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Isobutyl isothiocyanate → 1-[(2,4-Dimethoxybenzoyl)amino]-3-(2-methylpropyl)thiourea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isobutyl isothiocyanate | HCID 68960 | — |
| 反応物 | 2,4-Dimethoxybenzohydrazide | HCID 456728 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-[(2,4-Dimethoxybenzoyl)amino]-3-(2-methylpropyl)thiourea | HCID 2208428 | 90% |
反応手順
Ex-109B: A solution of 2,4-dimethoxy-benzoic acid hydrazide (Ex-109A, 1.0 g, 5.1 mmol) and isobutyl-isothiocyanate (0.70 g, 6.1 mmol) in ethanol (30 mL) was refluxed for 8 hours. The precipitate was filtered, washed with ethanol, dried in vacuo to afford 1-(2,4-dimethoxy-benzoyl)amino-3-isobutyl-thiourea (1.43 g). Additional product (0.1 g, 96% overall) was obtained by concentrating the mother liquid. 1H NMR (CDCl3) δ 10.71 (bs, 1H), 9.23 (bs, 1H), 8.03 (d, J=8.6 Hz, 1H), 6.98 (bs, 1H), 6.59 (dd, J=8.6, 2.6 Hz, 1H), 6.51 (d, J=2.6 Hz, 1H), 4.02 (s, 3H), 3.86 (s, 3H), 3.41 (dd, J=6.4, 6.6 Hz, 2H), 1.96–1.87 (m, 1H), 0.91 (d, J=6.5 Hz, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094801B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-8128df313cf4428687143d608ab819d6 |
| 出典メモ | uspto-grants-2006_08 |